Rapid trace level determination of sulfonamide residues in honey with online extraction using short C-18 column by high-performance liquid chromatography with fluorescence detection

被引:28
作者
Sajid, Muhammad [1 ]
Na, Na [1 ]
Safdar, Muhammad [2 ]
Lu, Xin [1 ,3 ]
Ma, Lin [1 ]
He, Lan [3 ]
Ouyang, Jin [1 ]
机构
[1] Beijing Normal Univ, Coll Chem, Beijing 100875, Peoples R China
[2] Natl Ctr Nanosci & Technol, Beijing 100190, Peoples R China
[3] Natl Inst Food & Drug Control, Beijing 100050, Peoples R China
关键词
Online extraction; C-18; extraction; Large volume injection; Sulfonamide; HPLC with fluorescence detection; Honey; TANDEM MASS-SPECTROMETRY; SOLID-PHASE EXTRACTION; ANTIBIOTIC-RESIDUES; SAMPLES;
D O I
10.1016/j.chroma.2013.09.020
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A sensitive and inexpensive quantification method with online extraction using a short C-18 column for sulfonamide residues in honey by high performance liquid chromatography with fluorescence detector was developed and validated. In sample preparation, acid hydrolysis was used to break the N-glycoside bond between the honey sugar and sulfonamide drugs and derivatization of sulfonamide residues with fluorescamine was conducted at pH 3.5 using a citrate buffer (0.5 M) in the honey matrix. The chromatography was carried out on Zorbax Extended C-18 (250 mm x 4.6 mm; 5 mu m) column, using a mixture of acetonitrile and an acetate buffer (pH 4.50, 20 mM) as a mobile phase. A Zorbax Extended C-18 (12 mm x 4.6 mm; 5 mu m) column was used for online extraction of fifteen sulfonamide residues from honey sample with the help of a two position valve. The limit of quantification of sulfonamide residues in honey was less than 3 ng g(-1), and the percentage recovery of study compounds in spiked honey sample was from 80% for sulfacetamide to 100% of sulfachloropyridazine. The developed method has excellent linearity for all studied sulfonamides with a correlation coefficient 0.993. (C) 2013 Elsevier B.V. All rights reserved.
引用
收藏
页码:173 / 179
页数:7
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